Ammonium Chloride → 5-Amino-2-[1,2,4]triazol-1-ylbenzonitrile
反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)=[C:8]([CH:11]=1)[C:9]#[N:10])([O-])=O.[Cl-].[NH4+].[In]>C(O)C>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)=[C:8]([CH:11]=1)[C:9]#[N:10]参加物
5
実験手順
5-Nitro-2-[1,2,4]triazol-1-yl-benzonitrile (1.14 g, 5.3 mmol) was dissolved in ethanol (23 mL) and satd. aq. ammonium chloride (5.3 mL) before adding indium powder (3.25 g, 28.2 mmol). The mixture was then refluxed for 3 h, cooled to RT, and the solids filtered (MeOH washed). The filtrate was diluted with water, basified with 1N NaOH (aq), and extracted with EtOAc. The organic layer was dried (Na2SO4), filtered, and concentrated under vacuum to yield the title compound (0.88 g). MS (ESI+) for m/z 186 (M+H)+.
後処理
- temperatureThe mixture was then refluxed for 3 h
- filtrationthe solids filtered
- wash(MeOH washed)
- additionThe filtrate was diluted with water
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-951b5b557a5a4b68ac799f381aa626f1
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07462600B2
反応ノート
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